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ChemicalBook CAS DataBase List 3-Methacryloxypropyltrimethoxysilane
2530-85-0

3-Methacryloxypropyltrimethoxysilane synthesis

9synthesis methods
tert-Butyl methyl ether

1634-04-4

(3-METHACRYLOYLOXYPROPYL)TRICHLOROSILANE

7351-61-3

3-Methacryloxypropyltrimethoxysilane

2530-85-0

A magnetic stir bar was placed into a 100-mL round-bottomed flask (Schlenk tube) equipped with a two-way stopper. Add 0.24 g (0.75 mmol) of bismuth trichloride (BiCl3) to the flask. The flask was sealed with a septum and nitrogen displacement was performed. Subsequently, 21.9 g (248 mmol) of methyl tert-butyl ether and 19.62 g (75 mmol) of 3-methacryloyloxypropyltrichlorosilane were added to the flask as in Example 1. The system was returned to room temperature (25°C). The reaction was carried out for 3 days (72 hours) under the stirring of a magnetic stirrer and the entire flask was required to be shaded with aluminum foil. Upon completion of the reaction, bismuth trichloride is removed by filtration through diatomaceous earth as it precipitates in the reaction solution. Finally, the yield of 3-(methacryloxy)propyltrimethoxysilane was determined. The experimental results were recorded in Table 2.

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Yield:2530-85-0 94.3%

Reaction Conditions:

with dihydrogen hexachloroplatinate;10H-phenothiazine at 85; under 1125.11 - 3000.3 Torr; for 4 h;Catalytic behavior;Autoclave;Inert atmosphere;Pressure;

Steps:

4 Embodiment 4

To a 2L autoclave equipped with a plunger metering pump inlet,Add 476.6g (3.90mol) of TMS,5.8 g of phenothiazine and 2.9 ml of Speier catalyst,Close the reaction vessel and start stirring.After replacing with nitrogen, it is heated to 85 ° C, and the kettle pressure is 0.15 MPa.365.8 g (2.90 mol) of AMA was slowly injected into the autoclave via a plunger metering pump to control the amount of injection.The kettle pressure is 0.2-0.4 MPa, and the injection time is about 2 hours.After the injection, the reaction was stirred at 85 ± 5 ° C for 2 hours.The temperature was lowered to room temperature, and after the pressure was released, the pale yellow reaction liquid was poured out.The reaction solution is subjected to fractional distillation under reduced pressure through a packed fractionation column (Φ2.5*100 cm, glass spring packing).Recover excess 110g of TMS,Collecting 679g of 120-125 ° C / 670-780Pa fraction,The yield was 94.30%, the purity was 99.78% (GC), and the high boiler was 30.1 g.

References:

CN108383868,2018,A Location in patent:Paragraph 0031; 0039; 0040

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